EP2412523A1 - Film flexible à base de polymere fluoré - Google Patents

Film flexible à base de polymere fluoré Download PDF

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Publication number
EP2412523A1
EP2412523A1 EP11177003A EP11177003A EP2412523A1 EP 2412523 A1 EP2412523 A1 EP 2412523A1 EP 11177003 A EP11177003 A EP 11177003A EP 11177003 A EP11177003 A EP 11177003A EP 2412523 A1 EP2412523 A1 EP 2412523A1
Authority
EP
European Patent Office
Prior art keywords
pvdf
layer
parts
film
composition
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Withdrawn
Application number
EP11177003A
Other languages
German (de)
English (en)
French (fr)
Inventor
Anthony Bonnet
Sandrine Duc
Cyrille Mathieu
Johann Laffargue
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Arkema France SA
Original Assignee
Arkema France SA
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Family has litigation
First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=37102975&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP2412523(A1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Arkema France SA filed Critical Arkema France SA
Publication of EP2412523A1 publication Critical patent/EP2412523A1/fr
Withdrawn legal-status Critical Current

Links

Classifications

    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/06—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B27/08—Layered products comprising a layer of synthetic resin as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/07—Flat, e.g. panels
    • B29C48/08—Flat, e.g. panels flexible, e.g. films
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/09—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels
    • B29C48/10—Articles with cross-sections having partially or fully enclosed cavities, e.g. pipes or channels flexible, e.g. blown foils
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B29C48/21—Articles comprising two or more components, e.g. co-extruded layers the components being layers the layers being joined at their surfaces
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29D—PRODUCING PARTICULAR ARTICLES FROM PLASTICS OR FROM SUBSTANCES IN A PLASTIC STATE
    • B29D7/00—Producing flat articles, e.g. films or sheets
    • B29D7/01—Films or sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B15/00—Layered products comprising a layer of metal
    • B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
    • B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B32—LAYERED PRODUCTS
    • B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/12—Layered products comprising a layer of synthetic resin next to a fibrous or filamentary layer
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    • B32B27/00—Layered products comprising a layer of synthetic resin
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    • B32B27/00—Layered products comprising a layer of synthetic resin
    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/304—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising vinyl halide (co)polymers, e.g. PVC, PVDC, PVF, PVDF
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    • B32B27/30—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers
    • B32B27/308—Layered products comprising a layer of synthetic resin comprising vinyl (co)polymers; comprising acrylic (co)polymers comprising acrylic (co)polymers
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    • B32B27/32—Layered products comprising a layer of synthetic resin comprising polyolefins
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/06—Interconnection of layers permitting easy separation
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    • B32B7/00—Layered products characterised by the relation between layers; Layered products characterised by the relative orientation of features between layers, or by the relative values of a measurable parameter between layers, i.e. products comprising layers having different physical, chemical or physicochemical properties; Layered products characterised by the interconnection of layers
    • B32B7/04—Interconnection of layers
    • B32B7/12—Interconnection of layers using interposed adhesives or interposed materials with bonding properties
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L27/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers
    • C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
    • C08L27/12—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment containing fluorine atoms
    • C08L27/16—Homopolymers or copolymers or vinylidene fluoride
    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
    • C08L33/00—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical, or of salts, anhydrides, esters, amides, imides or nitriles thereof; Compositions of derivatives of such polymers
    • C08L33/04—Homopolymers or copolymers of esters
    • C08L33/06—Homopolymers or copolymers of esters of esters containing only carbon, hydrogen and oxygen, which oxygen atoms are present only as part of the carboxyl radical
    • C08L33/10—Homopolymers or copolymers of methacrylic acid esters
    • C08L33/12—Homopolymers or copolymers of methyl methacrylate
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
    • H01L31/04—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof adapted as photovoltaic [PV] conversion devices
    • H01L31/042—PV modules or arrays of single PV cells
    • H01L31/048—Encapsulation of modules
    • H01L31/049—Protective back sheets
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/03—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor characterised by the shape of the extruded material at extrusion
    • B29C48/05—Filamentary, e.g. strands
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
    • B29C48/00—Extrusion moulding, i.e. expressing the moulding material through a die or nozzle which imparts the desired form; Apparatus therefor
    • B29C48/16—Articles comprising two or more components, e.g. co-extruded layers
    • B29C48/18—Articles comprising two or more components, e.g. co-extruded layers the components being layers
    • B29C48/22—Articles comprising two or more components, e.g. co-extruded layers the components being layers with means connecting the layers, e.g. tie layers or undercuts
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
    • B29K—INDEXING SCHEME ASSOCIATED WITH SUBCLASSES B29B, B29C OR B29D, RELATING TO MOULDING MATERIALS OR TO MATERIALS FOR MOULDS, REINFORCEMENTS, FILLERS OR PREFORMED PARTS, e.g. INSERTS
    • B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
    • B29K2027/12—Use of polyvinylhalogenides or derivatives thereof as moulding material containing fluorine
    • B29K2027/16—PVDF, i.e. polyvinylidene fluoride
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B2262/00—Composition or structural features of fibres which form a fibrous or filamentary layer or are present as additives
    • B32B2262/02—Synthetic macromolecular fibres
    • B32B2262/0223—Vinyl resin fibres
    • B32B2262/0238—Vinyl halide, e.g. PVC, PVDC, PVF, PVDF
    • B—PERFORMING OPERATIONS; TRANSPORTING
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    • B32B2262/02—Synthetic macromolecular fibres
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    • B32B2307/50—Properties of the layers or laminate having particular mechanical properties
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    • B82—NANOTECHNOLOGY
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    • Y10T442/2607—Radiation absorptive

Definitions

  • the present invention relates to a PVDF-based film for the protection of substrates and substrates covered by this film. It also relates to a multilayer structure associating a sheet of PET or PEN and the PVDF-based film. Finally, the invention relates to the uses of PVDF-based film or multilayer film, in particular for the protection of photovoltaic modules.
  • PVDF polyvinylidene fluoride
  • the Applicant has developed a PVDF-based film which has good flexibility and good tensile strength, which is usable in some applications. It has also developed a multilayer structure associating the PVDF-based film with a PET or PEN film.
  • Requirement EP 1382640 describes a film with two or three layers based on a PVDF homo- or copolymer.
  • the PVDF copolymer comprises 0 to 50% comonomer.
  • the examples describe the use of PVDF homopolymer.
  • Requirement EP 1566408 describes a film with two or three layers based on PVDF homo- or copolymer.
  • the PVDF copolymer comprises from 0 to 50% comonomer, advantageously from 0 to 25% and preferably from 0 to 15%.
  • the film does not contain any charge.
  • Requirement EP 172864 describes a photovoltaic cell protected by a PVDF / PET film. There is no adhesive layer between PVDF and PET.
  • the patent US 6555190 discloses a multilayer structure associating in the order a layer of PEN, an adhesive layer and a layer of a fluorinated polymer (PCTFE, PVDF, ).
  • the adhesive layer comprises a polyolefin functionalized with a carboxylic acid or an unsaturated anhydride or a homo- or copolymer comprising, as monomer (s), acrylic acid, alkyl acrylates and acrylates optionally modified with an unsaturated acid or anhydride.
  • Requirement US 2005/0268961 discloses a film-protected photovoltaic module comprising two fluoropolymer layers, one having a melting temperature greater than 135 ° C, the other having a melting temperature of less than 135 ° C.
  • the invention relates to a multilayer structure using a PVDF-based film as defined in claim 1.
  • the invention also relates to the uses of this structure and to the process for manufacturing a PVDF-based film.
  • PVDF PVDF
  • the VDF contains, by weight, at least 50% of VDF, more preferably at least 75% and more preferably at least 85%.
  • a PVDF advantageously comprising by weight 5 to 20%, advantageously 7 to 13%, of at least one fluorinated comonomer for 80 to 95% of VDF, advantageously for 87 to 93% of VDF (hereinafter referred to as this type of PVDF by "flexible PVDF").
  • the flexible PVDF is used for compositions A and B.
  • the fluorinated comonomer copolymerizable with VDF is chosen for example from vinyl fluoride; trifluoroethylene (VF3); chlorotrifluoroethylene (CTFE); 1,2-difluoroethylene; tetrafluoroethylene (TFE); hexafluoropropylene (HFP); perfluoro (alkyl vinyl) ethers such as perfluoro (methyl vinyl) ether (PMVE), perfluoro (ethyl vinyl) ether (PEVE) and perfluoro (propyl vinyl) ether (PPVE); perfluoro (1,3-dioxole); perfluoro (2,2-dimethyl-1,3-dioxole) (PDD).
  • VF3 trifluoroethylene
  • CTFE chlorotrifluoroethylene
  • TFE tetrafluoroethylene
  • HFP hexafluoropropylene
  • perfluoro (alkyl vinyl) ethers such as perfluor
  • the fluorinated comonomer is chosen from chlorotrifluoroethylene (CTFE), hexafluoropropylene (HFP), trifluoroethylene (VF3) and tetrafluoroethylene (TFE).
  • CTFE chlorotrifluoroethylene
  • HFP hexafluoropropylene
  • VF3 trifluoroethylene
  • TFE tetrafluoroethylene
  • the comonomer is advantageously HFP because it copolymerizes well with VDF and provides good thermomechanical properties.
  • the copolymer comprises only VDF and HFP.
  • the PVDF has a viscosity ranging from 100 Pa.s to 2000 Pa.s, the viscosity being measured at 230 ° C., at a shear rate of 100 s -1 using a capillary rheometer.
  • this type of PVDF is well suited to extrusion.
  • the PVDF has a viscosity ranging from 300 Pa.s to 1200 Pa.s, the viscosity being measured at 230 ° C., at a shear rate of 100 s -1 using a capillary rheometer.
  • MMA methyl methacrylate
  • copolymers containing at least 50% by weight of MMA and at least one other monomer copolymerizable with MMA are thus designated.
  • alkyl (meth) acrylates examples include alkyl (meth) acrylates, acrylonitrile, butadiene, styrene and isoprene.
  • alkyl (meth) acrylates are described in KIRK-OTHMER, Encyclopedia of Chemical Technology, 4th Edition in Vol. 1 pages 292-293 and in the Flight. 16 pages 475-478 .
  • the PMMA comprises, by weight, from 0 to 20% and preferably 5 to 15% of a C 1 -C 8 alkyl (meth) acrylate, which is preferably methyl acrylate and / or ethyl acrylate.
  • PMMA can be functionalized, that is to say it contains, for example, acid, acid chloride, alcohol, anhydride functions. These functions can be introduced by grafting or by copolymerization.
  • it is an acid function provided by the acrylic acid comonomer. Two neighboring acrylic acid functions may dehydrate to form an anhydride.
  • the proportion of functions can be from 0 to 15% by weight of the PMMA including the possible functions.
  • PMMA may optionally comprise at least one acrylic elastomer but it is preferable to avoid using such a PMMA because the acrylic elastomer can induce bleaching of the film.
  • acrylic elastomer There are commercial grades of "shock" PMMA which contain an acrylic elastomer in the form of multilayer particles. The acrylic elastomer is then present in the PMMA as it is marketed (that is to say introduced into the resin during the manufacturing process) but it can also be added during the manufacture of the film.
  • the proportion of acrylic elastomer ranges from 0 to 30 parts for 70 to 100 parts of PMMA, the total being 100 parts.
  • the multilayer particles also commonly known as core-shell, may be used as acrylic elastomer, they comprise at least one elastomeric (or soft) layer, ie a layer formed of a polymer having a glass transition temperature (Tg) less than -5 ° C and at least one rigid (or hard) layer, that is to say formed of a polymer having a Tg greater than 25 ° C.
  • the size of the particles is generally less than 1 ⁇ m and advantageously between 50 and 300 nm. Examples of core-shell multilayer particles can be found in the following documents: EP 1061100 A1 , US 2004/0030046 A1 , FR-A-2446296 or US 2005/0124761 A1 . Particles having at least 80% by weight of soft elastomeric phase are preferred.
  • the function of the acrylic elastomer is to improve the tensile strength of PMMA (impact modifier) and to promote the flexibility of PMMA.
  • the MVI (melt volume index or melt volume index in the molten state) of the PMMA may be between 2 and 15 cm 3/10 min measured at 230 ° C under a load of 3.8 kg.
  • the adhesive layer makes it possible to adhere the film to the substrate and consists of any type of adhesive making it possible to adhere the film to the substrate.
  • the urethane (PU-adhesive), epoxy, acrylic or polyester glues can be used for the adhesive layer, whether in thermoplastic or thermosetting form.
  • PU glue it will be possible to use a PU glue.
  • UV absorber it may be for example the additives mentioned in the patent US 5256472 .
  • Benzotriazole, benzophenone, benzylidene malonate or quinazoline compounds are advantageously used.
  • the dispersing agent its function is to help disperse the mineral filler.
  • It is preferably a polyalkylene glycol, i.e. a polymer containing alkylene oxide units (eg ethylene oxide or propylene oxide).
  • poly (oxyethylene) glycol called commonly polyethylene glycol (PEG).
  • the polyalkylene glycol preferably has a number average mass of between 1000 and 10000 g / mol.
  • the polyalkylene glycol makes it possible to coat the particles of the mineral filler and to avoid direct contact between the particles and the PVDF.
  • the mineral filler may be a metal oxide such as, for example, titanium dioxide (TiO 2 ), silica, quartz, alumina, a carbonate such as, for example, calcium, talc, mica, dolominte (CaCO 3 • MgCO 3 ), montmorillonite (aluminosilicate), BaSO 4 , ZrSiO 4 , Fe 3 O 4 .
  • TiO 2 titanium dioxide
  • silica silica
  • quartz quartz
  • alumina a carbonate
  • carbonate such as, for example, calcium, talc, mica, dolominte (CaCO 3 • MgCO 3 ), montmorillonite (aluminosilicate), BaSO 4 , ZrSiO 4 , Fe 3 O 4 .
  • the mineral filler has an opacifying function in the UV / visible range.
  • the protective action of the charge is complementary to that of the UV absorber.
  • the opacifying mineral filler retains a protective action longer (it is not degraded).
  • a charge of TiO 2 is particularly preferred from this point of view.
  • the mineral filler may have another function.
  • it may be a flame retardant filler, such as, for example, antimony oxide (Sb 2 O 3 , Sb 2 O 5 ) Al (OH) 3 , Mg (OH) 2 , huntite (3MgCO 3 • CaCO 3 ), hydromagnesite (3MgCO 3 • Mg (OH) 2 • 3H 2 O).
  • It can also be a conductive charge of electricity (for example, carbon black or carbon nanotubes).
  • the filler has a size generally between 0.05 ⁇ m and 1 mm.
  • the content of inorganic filler in composition A or C is between 0.1 and 30 parts (for a total of 100 parts).
  • the content varies between 10 and 25 parts, preferably between 10 and 20 parts.
  • the mineral filler content is at least 10 parts to observe a good effectiveness of the opacifying filler (and possibly flame retardant). It is also preferable that this content does not exceed 25 parts, or even 20 parts, so as not to degrade the mechanical properties of the layer which comprises the charge, and therefore the mechanical properties of the entire film.
  • PVDF-based film As regards the PVDF-based film , it comes in several forms.
  • Composition A comprises from 50 to 70 parts of at least one PVDF, from 10 to 40 parts of at least one PMMA and from 10 to 25 parts of at least one mineral filler (preferably TiO 2 ), the total doing 100 parts.
  • the PVDF of composition A is a flexible PVDF.
  • the PVDF of composition B is a flexible PVDF.
  • the composition B does not contain any acrylic elastomer or core-shell particle.
  • Composition C comprises only PVDF as polymer.
  • Composition A comprises from 50 to 70 parts of at least one PVDF, from 10 to 40 parts of minus one PMMA and from 10 to 25 parts of at least one mineral filler (preferably TiO 2 ), the total being 100 parts.
  • the PVDF of composition C is a PVDF homopolymer.
  • the PVDF of composition A is a flexible PVDF.
  • Composition C comprises only polymer as PVDF.
  • Composition B comprises from 5 to 40 parts of at least one PVDF, from 60 to 95 parts of at least one PMMA and from 0 to 5 parts of at least one UV absorber, the total being 100 parts.
  • Composition A comprises from 50 to 70 parts of at least one PVDF, from 10 to 40 parts of at least one PMMA and from 10 to 25 parts of at least one mineral filler (preferably TiO 2 ), the total doing 100 parts.
  • the PVDF of composition C is a PVDF homopolymer.
  • the PVDF of composition A and / or B is a flexible PVDF.
  • the layer of composition C which is disposed against the layer of composition A, is the most "external" layer.
  • composition A and / or B preferably does not contain any acrylic elastomer or core-shell particle. Indeed, this can induce a bleaching of the film when the latter is subjected to deformation important, which is the case for example during the manufacture of the film is during the introduction of the film on the substrate (for example during the stamping of a sheet of metal protected by the film).
  • the PVDF-based film which protects the substrate therefore comprises, in order from the substrate, a layer of optional composition B, a layer of composition A, a layer of composition C, the film adhering to the substrate by an adhesive layer and if the composition layer B is present, the adhesive layer is optional.
  • the thickness of the composition layer A is preferably between 5 and 50 ⁇ m, preferably between 5 and 15 ⁇ m.
  • the thickness of the layer of composition B is preferably between 5 and 45 microns, preferably between 5 and 15 microns.
  • the thickness of the layer of composition C is preferably between 2 and 30 microns, preferably between 2 and 15 microns.
  • the PVDF film is preferably manufactured by the coextrusion technique, but it is also possible to use a solvent processing technique or by using the plaxing technique.
  • the PVDF-based film can also be manufactured by coextrusion-blowing film ("blown film").
  • blown film This technique consists in extruding, generally from bottom to top, a thermoplastic polymer through an annular die, the extrudate is simultaneously drawn longitudinally by a drawing device, usually in rolls, and inflated by a constant volume of air trapped between the die, the draw system and the wall of the sheath.
  • the inflated sheath also called “bubble” is generally cooled by an air blowing ring at the exit of the die.
  • the flat bubble is rolled up, either in the form of a sheath or after cutting into two separate films.
  • a semi-crystalline fluid polymer is coextruded with a thermoplastic resin which is incompatible such that after cooling and flattening of the bubble, the two extruded films are recovered separately by conventional means, such as by separate winding separate films.
  • a bubble consists of a film of 25 microns of PVDF coextruded with a film of 60 microns of polyethylene (PE).
  • PE polyethylene
  • the thickness of the PE film should preferably be 1 to 5 times the thickness of the semi-crystalline polymer film. It is also written that it is not excluded to coextrude more than two films, but nothing is specified on the exact nature of the films in question.
  • International demand WO 03/039840 discloses a process for producing a fluorinated film which also uses an incompatible polymer, which may be PE, impact polystyrene, plasticized PVC and preferably low density PE.
  • the polyolefin (also called “liner”) used in b) may be the same or different from that used in c).
  • Photovoltaic modules can be protected at the rear by the PVDF-based film.
  • a photovoltaic module makes it possible to convert light energy into electric current.
  • a photovoltaic module comprises photovoltaic cells mounted in series and connected together by means of electrical connection.
  • Photovoltaic cells are generally mono junction fabricated based on multi-crystalline silicon doped "P” with boron during the melting of silicon and doped "N” with phosphorus on their illuminated surface. These cells are put in place in a laminated stack.
  • the laminated stack may consist of EVA (ethylene-vinyl acetate copolymer) coating photovoltaic cells to protect silicon from oxidation and moisture.
  • the stack is nested between a glass plate that serves as a support on one side and is protected by a film on the other side.
  • the photovoltaic module is thus protected against aging (UV, salt spray, etc.) against scratches, moisture or water vapor
  • both F1 and F2 films are as defined above. They may be identical or different, that is to say they may be independently of one another according to one of the four forms of the invention described. previously.
  • Each of the two films F1 or F2 adheres to the PET sheet using a layer of composition B or using an adhesive layer.
  • the adhesive layer does not comprise any polyolefin functionalized with a carboxylic acid or an unsaturated anhydride or else a homo- or copolymer comprising, as monomer (s), acrylic acid, alkyl acrylates and acrylates optionally modified with an acid. or anhydride unsaturated.
  • compositions A and / or B contain no acrylic elastomer or core-shell particle.
  • the multilayer structure can be manufactured by hot compression of the various elements (that is to say the PET sheet, the film (s) based on PVDF, ). It is also possible to use the lamination technique which consists of continuously rolling the PVDF-based film (s) (previously in the form of a coil) with the PET film on which the adhesive was optionally deposited.
  • An example of a vacuum lamination process for applying a type of structure or ICOSOLAR AKASOL ® ® on a photovoltaic module is disclosed in US 5593532 and can be applied to the multilayer structure of the invention.
  • the structure is manufactured by combining the PVDF-based film (s) already formed with the PET film.
  • the adhesive layer comprises a polyolefin functionalized with a carboxylic acid or an unsaturated anhydride or a homo- or copolymer comprising, as monomer (s), acrylic acid, alkyl acrylates and acrylates optionally modified with an unsaturated acid or anhydride.
  • PET polyethylene naphthalate
  • PET polyethylene naphthalate
  • PEN has excellent UV resistance but PEN films are brittle and are not moisture barrier.
  • Figures 1 and 2 show schematically examples of a photovoltaic module 2 protected.
  • Reference 3 in FIG. 1 represents either a PVDF-based film or a multilayer structure associating a sheet of PET or PEN with one or two PVDF-based films.
  • the invention also relates to the photovoltaic module protected by the PVDF-based film or by the multilayer structure.
  • the following order is therefore: (the module) / adhesive layer / comp. B vent. / comp. A / comp. C vent.,
  • the adhesive layer being optional if the composition layer B is present.
  • the invention is however not limited to the photovoltaic module as described above or in FIG. 2.
  • Other examples of photovoltaic modules will thus be found in FR 2863775 A1 (see in particular Figure 1), US 6369316 B1 , US 2004/0229394 A1 , US 2005/0172997 A1 , US 2005/0268961 A1 .
  • the PVDF-based film can be used to protect a flexible substrate such as a technical textile that can be woven or non-woven. It may be a fabric made of PVC, polyester or polyamide, a glass fabric, a glass mat, a fabric of aramid or Kevlar, ....
  • a PVC tarpaulin is an example of a flexible substrate in PVC.
  • the film of the invention may be for example applied to the technical fabric using the lamination technique or by coating.
  • the invention also relates to the technical textile protected by the film based on PVDF.
  • the adhesive layer being optional if the composition layer B is present.
  • the PVDF-based film can be colaminated on a metal substrate which can be for example steel, copper or aluminum. Preferably, it is a metal sheet, preferably steel. Preferably, the steel is galvanized, and is coated or not with a primer. For example, the steel can be treated with Zincrox or coated with B1236 acrylic / vinyl primer, B710 epoxy primer or CN4118 melamine polyester primer.
  • the PVDF-based film is sufficiently flexible so that the steel / film assembly can then undergo significant deformation. For example, the set can be stamped.
  • FIG. 3 represents an example of a piece of steel 10 protected by the PVDF-based film, referenced 10.
  • the part represents a metal cup (for example made of steel) obtained by stamping a sheet of metal on which was colaminated the movie.
  • the invention also relates to the metal substrate protected by the PVDF-based film.
  • the adhesive layer being optional if the composition layer B is present.
  • PVDF-1 VDF / HFP copolymer in the form of granules (10% HFP by weight) MVI of 1.1 cm 3/10 min (230 ° C, 5 kg), having a viscosity of 2500 mPa s at 230 ° C, 100 s -1 and a melting temperature of about 145 ° C.
  • Altuglas ® BS 580 (previously sold as OROGLAS ® BS8): PMMA company INTERNATIONAL Altuglas (formerly Atoglas) MVI 4.5 cm 3/10 min (230 ° C, 3.8 kg) in the form of beads containing a comonomer, methyl acrylate at a level of 6% by weight. This PMMA does not contain a shock additive or acrylic elastomer.
  • PVDF-2 PVDF homopolymer granulated MVI of 1.1 cm 3/10 min (230 ° C, 5 kg).
  • PVDF-3 VDF / HFP copolymer in pellet form (17 weight% HFP) MVI 10 cm 3/10 min (230 ° C, 5 kg), having a viscosity of 900 mPa s at 230 ° C, 100 s - 1 .
  • DESMODUR ® N-100 aliphatic isocyanate of CAS No. 28182-81-2 marketed by LANXESS.
  • FLUORAD ® FC-430 fluorinated surfactant from 3M.
  • TONE ® 201 poly (caprolactone) diol marketed by Union Carbide (molecular weight approximately 830 g / mol).
  • Example 1 (according to the invention, 1 era form)
  • a monolayer film consisting of 60 wt% of PVDF-1, 15% of TiO 2 R960 reference and 25% of Altuglas BS ® 580 is extruded as a film thickness of 15 microns and width 2000 mm using a film extruder at a temperature of 245 ° C.
  • DBTL dibutyl tin dilaurate b
  • the monolayer film is then laminated at 130 ° C on the polyester substrate (thus obtaining a PET / PU glue / monolayer film structure).
  • the adhesion obtained is greater than 40 N / cm. After a passage of 8 hours in an oven at 95 ° C the adhesion is retained, the structure can be folded easily without generating a crack in the fluorinated film.
  • Example 2 (according to the invention, 3 th form)
  • the adhesion obtained is greater than 60 N / cm. After a passage of 8 hours in an oven at 95 ° C, the adhesion is retained, the structure can be folded easily without generating a crack in the fluorinated film.
  • Example 3 (according to the invention, 1 era form)
  • DBTL dibutyl tin dilaurate b
  • FC-430 10% fluorinated surfactant
  • the monolayer film is then laminated at 130 ° C on the polyester substrate (thus obtaining a PET / PU glue / monolayer film structure).
  • the adhesion obtained is greater than 40 N / cm. After a passage of 8 hours in an oven at 95 ° C, the adhesion is retained, the structure can be folded easily without generating a crack in the fluorinated film. This film also has excellent fire resistance.
  • Example 4 (according to the invention, 1 era form)
  • DBTL dibutyl tin dilaurate b
  • FC-430 10% fluorinated surfactant
  • the two-layer structure is then laminated at 130 ° C. on the polyester substrate, the layer in contact with the PU adhesive being that containing the PVDF-3.
  • the layer in contact with the PU adhesive being that containing the PVDF-3.
  • a PET / PU glue / monolayer film complex containing PVDF-3 is thus obtained, and protected by the PE layer which can then be removed simply before use of the complex.
  • the adhesion obtained between the PET and the PVDF-based film is greater than 40 N / cm. After a passage of 8 hours in an oven at 95 ° C, the adhesion is retained, the structure can be folded easily without generating a crack in the fluorinated film. This film also has excellent fire resistance.

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EP11177003A 2006-01-25 2007-01-25 Film flexible à base de polymere fluoré Withdrawn EP2412523A1 (fr)

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FR0600695A FR2896445B1 (fr) 2006-01-25 2006-01-25 Film flexible a base de polymere fluore
EP07731521A EP1979162A2 (fr) 2006-01-25 2007-01-25 Film flexible a base de polymere fluore

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JP5274994B2 (ja) 2013-08-28
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JP5611303B2 (ja) 2014-10-22
WO2007085769A3 (fr) 2007-09-13
CN101410249A (zh) 2009-04-15
US20090275251A1 (en) 2009-11-05
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CN102862359A (zh) 2013-01-09
KR20090126331A (ko) 2009-12-08
JP2009524537A (ja) 2009-07-02
FR2896445B1 (fr) 2010-08-20
WO2007085769A2 (fr) 2007-08-02
FR2896445A1 (fr) 2007-07-27
CN101518972A (zh) 2009-09-02
JP2009078559A (ja) 2009-04-16
CN101410249B (zh) 2012-09-05
EP1979162A2 (fr) 2008-10-15
KR101016933B1 (ko) 2011-02-25
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JP2013056547A (ja) 2013-03-28
CN101518972B (zh) 2013-04-17

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